Encapsulation is a means by which bioactives can be protected and incorporated into processed foods. Oil-protein-carbohydrate microcapsules were formulated to contain 0.025% - 50% bioactives. A reliable analytical method was developed for quantifying the level of bioactives to verify content claims of microencapsulated ingredients. DMSO can be used to rapidly extract a variety of encapsulated bioactives from lipid-protein-carbohydrate matrices. The encapsulant matrix is completely and rapidly dissolved in heated DMSO. This methodology has been applied to encapsulated a-tocopherol, trans-resveratrol and curcumin. The resultant DMSO extract is injected directly onto either a normal phase (NP) or a reversed phase (RP) column, fitted with matching guard columns, followed by either photo diode array or fluorescence detection.